A new catalyst, Sm2NdSbO7, was synthesized for the first time by solid-phase sintering. The study utilized X-ray diffraction, transmission electron microscope energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy to examine the structural characteristics of monocrystal BiDyO3, monocrystal Sm2NdSbO7 and Sm2NdSbO7/BiDyO3 heterojunction photocatalysts (SBHP) prepared by solid-phase sintering. The Sm2NdSbO7 photocatalyst owned a pyrochlorite structure, belonged to the face-centered cubic crystal system, possessed a space group of Fd3m and a bandgap width of 2.750 eV. After 145 min of visible light irradiation (145-VLIRD), the removal rate (RMR) of methyl parathion (MP) or total organic carbon of SBHP was 100% or 97.58%, respectively. After 145-VLIRD, the photocatalytic degradation rates of SBHP to MP were 1.13 times, 1.20 times, and 2.43 times higher than those of the Sm2NdSbO7 photocatalyst, the BiDyO3 photocatalyst, and the nitrogen-doped TiO2 catalyst, respectively. The experimental results showed that SBHP had good photocatalytic activity. After four cycles of cyclic degradation experiments with SBHP, the elimination rates of MP were 98.76%, 97.44%, 96.32%, and 95.72%, respectively. The results showed that SBHP had good stability. Finally, the possible degradation pathways and degradation mechanisms of MP were speculated. In this study, we successfully developed a high-efficiency heterojunction catalyst which responded to visible light and possessed significant photocatalytic activity. The catalyst could be used in photocatalytic reaction system for eliminating the harmful organic pollutants from wastewater.